CN109397724A - A kind of high temperature resistant composite and its high-temperature heat expansion forming method - Google Patents
A kind of high temperature resistant composite and its high-temperature heat expansion forming method Download PDFInfo
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- CN109397724A CN109397724A CN201811404850.2A CN201811404850A CN109397724A CN 109397724 A CN109397724 A CN 109397724A CN 201811404850 A CN201811404850 A CN 201811404850A CN 109397724 A CN109397724 A CN 109397724A
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- high temperature
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- resistant composite
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- 238000000034 method Methods 0.000 title claims abstract description 69
- 239000002131 composite material Substances 0.000 title claims abstract description 51
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 27
- 239000003292 glue Substances 0.000 claims abstract description 17
- 229920001971 elastomer Polymers 0.000 claims abstract description 11
- 238000010438 heat treatment Methods 0.000 claims abstract description 7
- 238000009413 insulation Methods 0.000 claims abstract description 5
- 239000011347 resin Substances 0.000 claims description 25
- 229920005989 resin Polymers 0.000 claims description 25
- 239000004744 fabric Substances 0.000 claims description 16
- 239000000835 fiber Substances 0.000 claims description 15
- 239000000463 material Substances 0.000 claims description 12
- 229920000049 Carbon (fiber) Polymers 0.000 claims description 9
- 239000004917 carbon fiber Substances 0.000 claims description 9
- 239000011159 matrix material Substances 0.000 claims description 8
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 8
- 230000002787 reinforcement Effects 0.000 claims description 8
- 229920001721 polyimide Polymers 0.000 claims description 7
- 238000004073 vulcanization Methods 0.000 claims description 7
- 239000011521 glass Substances 0.000 claims description 6
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims description 5
- XLJMAIOERFSOGZ-UHFFFAOYSA-M cyanate Chemical compound [O-]C#N XLJMAIOERFSOGZ-UHFFFAOYSA-M 0.000 claims description 5
- 239000003822 epoxy resin Substances 0.000 claims description 5
- 229910052731 fluorine Inorganic materials 0.000 claims description 5
- 239000011737 fluorine Substances 0.000 claims description 5
- 229920005560 fluorosilicone rubber Polymers 0.000 claims description 5
- LNEPOXFFQSENCJ-UHFFFAOYSA-N haloperidol Chemical compound C1CC(O)(C=2C=CC(Cl)=CC=2)CCN1CCCC(=O)C1=CC=C(F)C=C1 LNEPOXFFQSENCJ-UHFFFAOYSA-N 0.000 claims description 5
- 150000002978 peroxides Chemical class 0.000 claims description 5
- 229920000647 polyepoxide Polymers 0.000 claims description 5
- 239000010453 quartz Substances 0.000 claims description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 5
- 239000004753 textile Substances 0.000 claims description 5
- OMPJBNCRMGITSC-UHFFFAOYSA-N Benzoylperoxide Chemical compound C=1C=CC=CC=1C(=O)OOC(=O)C1=CC=CC=C1 OMPJBNCRMGITSC-UHFFFAOYSA-N 0.000 claims description 4
- 229920001774 Perfluoroether Polymers 0.000 claims description 4
- 235000019400 benzoyl peroxide Nutrition 0.000 claims description 4
- 238000004132 cross linking Methods 0.000 claims description 4
- 239000003365 glass fiber Substances 0.000 claims description 4
- 239000012948 isocyanate Substances 0.000 claims description 4
- 150000002513 isocyanates Chemical class 0.000 claims description 4
- 239000009719 polyimide resin Substances 0.000 claims description 4
- XMNIXWIUMCBBBL-UHFFFAOYSA-N 2-(2-phenylpropan-2-ylperoxy)propan-2-ylbenzene Chemical compound C=1C=CC=CC=1C(C)(C)OOC(C)(C)C1=CC=CC=C1 XMNIXWIUMCBBBL-UHFFFAOYSA-N 0.000 claims description 3
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims 3
- PEEHTFAAVSWFBL-UHFFFAOYSA-N Maleimide Chemical compound O=C1NC(=O)C=C1 PEEHTFAAVSWFBL-UHFFFAOYSA-N 0.000 claims 1
- 230000007547 defect Effects 0.000 abstract description 4
- 230000032683 aging Effects 0.000 abstract description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 abstract description 2
- 229910052710 silicon Inorganic materials 0.000 abstract description 2
- 239000010703 silicon Substances 0.000 abstract description 2
- 238000004321 preservation Methods 0.000 description 8
- 238000007711 solidification Methods 0.000 description 8
- 230000008023 solidification Effects 0.000 description 8
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 6
- 229910052799 carbon Inorganic materials 0.000 description 6
- 238000000465 moulding Methods 0.000 description 6
- 229920002379 silicone rubber Polymers 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
- 239000004642 Polyimide Substances 0.000 description 3
- 239000000654 additive Substances 0.000 description 3
- 230000000996 additive effect Effects 0.000 description 3
- 239000011248 coating agent Substances 0.000 description 3
- 238000000576 coating method Methods 0.000 description 3
- 229920001973 fluoroelastomer Polymers 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- OKIRBHVFJGXOIS-UHFFFAOYSA-N 1,2-di(propan-2-yl)benzene Chemical compound CC(C)C1=CC=CC=C1C(C)C OKIRBHVFJGXOIS-UHFFFAOYSA-N 0.000 description 2
- MJSQSKNNMZQLQZ-UHFFFAOYSA-N 1-butylperoxy-2-propan-2-ylbenzene Chemical compound CCCCOOC1=CC=CC=C1C(C)C MJSQSKNNMZQLQZ-UHFFFAOYSA-N 0.000 description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 2
- 239000005864 Sulphur Substances 0.000 description 2
- 239000000805 composite resin Substances 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 239000004643 cyanate ester Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 150000003949 imides Chemical class 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 230000035882 stress Effects 0.000 description 2
- 238000010792 warming Methods 0.000 description 2
- WVGXBYVKFQJQGN-UHFFFAOYSA-N 1-tert-butylperoxy-2-propan-2-ylbenzene Chemical class CC(C)C1=CC=CC=C1OOC(C)(C)C WVGXBYVKFQJQGN-UHFFFAOYSA-N 0.000 description 1
- 125000003903 2-propenyl group Chemical group [H]C([*])([H])C([H])=C([H])[H] 0.000 description 1
- 239000004952 Polyamide Substances 0.000 description 1
- 125000002252 acyl group Chemical group 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 230000009970 fire resistant effect Effects 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229920002647 polyamide Polymers 0.000 description 1
- 230000002028 premature Effects 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000005486 sulfidation Methods 0.000 description 1
- KSEOCVXHTQESHA-UHFFFAOYSA-N tricyanatomethyl cyanate Chemical compound N#COC(OC#N)(OC#N)OC#N KSEOCVXHTQESHA-UHFFFAOYSA-N 0.000 description 1
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C70/00—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts
- B29C70/04—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts comprising reinforcements only, e.g. self-reinforcing plastics
- B29C70/28—Shaping operations therefor
- B29C70/40—Shaping or impregnating by compression not applied
- B29C70/42—Shaping or impregnating by compression not applied for producing articles of definite length, i.e. discrete articles
- B29C70/46—Shaping or impregnating by compression not applied for producing articles of definite length, i.e. discrete articles using matched moulds, e.g. for deforming sheet moulding compounds [SMC] or prepregs
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C35/00—Heating, cooling or curing, e.g. crosslinking or vulcanising; Apparatus therefor
- B29C35/02—Heating or curing, e.g. crosslinking or vulcanizing during moulding, e.g. in a mould
- B29C35/0288—Controlling heating or curing of polymers during moulding, e.g. by measuring temperatures or properties of the polymer and regulating the process
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C70/00—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts
- B29C70/04—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts comprising reinforcements only, e.g. self-reinforcing plastics
- B29C70/28—Shaping operations therefor
- B29C70/54—Component parts, details or accessories; Auxiliary operations, e.g. feeding or storage of prepregs or SMC after impregnation or during ageing
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C70/00—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts
- B29C70/68—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts by incorporating or moulding on preformed parts, e.g. inserts or layers, e.g. foam blocks
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/14—Peroxides
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Composite Materials (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Physics & Mathematics (AREA)
- Oral & Maxillofacial Surgery (AREA)
- Thermal Sciences (AREA)
- Organic Chemistry (AREA)
- Polymers & Plastics (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Casting Or Compression Moulding Of Plastics Or The Like (AREA)
- Laminated Bodies (AREA)
- Moulds For Moulding Plastics Or The Like (AREA)
Abstract
The present invention relates to a kind of high temperature resistant composite and its high-temperature heat expansion forming methods.The forming method includes the following steps: to prepare fluorubber core model: fluorubber and vulcanizing agent being uniformly mixed, deaeration is configured to glue；The master mold of soft mode is processed according to element structure design requirement；Glue is poured into master mold to vulcanize, obtains fluorubber core model；Wherein, the mass ratio of the fluorubber and the vulcanizing agent is 100:(7~10)；(2) prepreg is processed into prefabricated component, placed the preform between fluorubber core model and former, determined process gap, then mold, fastened；Die cavity and prefabricated component therein to mold carry out vacuumize process, then carry out heating and thermal insulation to mold, are finally solidified, obtain the high temperature resistant composite.This method solve traditional silicon ageing of rubber under the high temperature conditions, and the bulbs of pressure to be caused to reduce, and solidifying pressure not enough causes product the defects of loose occur.
Description
Technical field
The present invention relates to technical field of composite material molding more particularly to a kind of high temperature resistant composite and its high warm are swollen
Swollen forming method.
Background technique
Thermal expansion technique refer to material prepreg in being closed rigid former by the thermal expansion of silicon rubber core model come
It realizes and cured forming method is processed to multiple platform material.Effectively and reasonably control silicon rubber thermal expansion stresses be thermal expansion at
Key technology in type technique, therefore current research emphasis focuses primarily on the thermal expansion for how controlling silicon rubber in forming process
In pressure.The core model of traditional thermal expansion technique mainly uses silicon rubber, and core model can generate the bulbs of pressure of all directions, be not necessarily to
External pressure source, the molding especially suitable for complicated composite element.But as the solidification temperature of composite material constantly mentions
Height, traditional silicon rubber mandrel under high temperature environment can rapid aging, surface generates micro-crack and the embrittlement that is hardened, can not effectively mention
Thermal expansion pressure.Therefore, composite material molding for hot setting, traditional thermal expansion technique can not be competent at.
In view of this, the present invention is specifically proposed.
Summary of the invention
The purpose of the present invention is to provide a kind of to can produce comprehensive, multi-angle foot within the scope of the pressed temperature of design
Enough pressure, the co-curing suitable for Multicarity high temperature resistant composite product form, and gained product intensity is high, good appearance, fits
Size is closed, can satisfy design requirement.
In order to solve to realize above-mentioned purpose, the present invention provides the following technical scheme that
1, a kind of high temperature resistant composite high-temperature heat expansion forming method, includes the following steps:
(1) prepare fluorubber core model: fluorubber and vulcanizing agent being uniformly mixed, deaeration is configured to glue；According to component knot
Structure design requirement processes the master mold of soft mode；Glue is poured into master mold to vulcanize, obtains fluorubber core model；Wherein, the fluorine
The mass ratio of rubber and the vulcanizing agent is 100:(7~10)；
(2) prepreg is processed into prefabricated component, places the preform between fluorubber core model and former, determines technology room
Then gap molds, fastening；
(3) vacuumize process is carried out to the die cavity of mold and prefabricated component therein, heating and thermal insulation then is carried out to mold,
Finally solidified, obtains the high temperature resistant composite.
2, high temperature resistant composite high-temperature heat expansion forming method according to technical solution 1, the fluorubber use
Fluorine silicone rubber and/or fluoroether rubber.
3, the high temperature resistant composite high-temperature heat expansion forming method according to technical solution 2,120~150 DEG C into
The row vulcanization, time controlled at 60~80 minutes.
4, according to the described in any item high temperature resistant composite high-temperature heat expansion forming methods of technical solution 1 to 3, the sulphur
Agent is using the peroxide that can carry out cross-linking reaction with fluorubber at 80 DEG C or less；Preferably, the vulcanizing agent is selected from peroxide
Change diisopropylbenzene (DIPB), peroxidating bis- (2,4 dichloro benzene formyls), dibenzoyl peroxide, double tert-butyl peroxy cumenes, three allyls
Based isocyanate is any one or more of.
5, high temperature resistant composite high-temperature heat expansion forming method according to technical solution 1, the process gap are
1.3~1.5mm.
6, high temperature resistant composite high-temperature heat expansion forming method according to technical solution 1, the prepreg include
Resin matrix and fibre reinforcement；Preferably, the resin matrix carrys out acyl selected from High temperature epoxy resins, cyanate resin, span
Imide resin, polyimide resin are any one or more of；Preferably, the fibre reinforcement is selected from carbon fibre fabric, glass
Glass fabric, quartz textile, carbon fiber, glass fibre are any one or more of.
7, high temperature resistant composite high-temperature heat expansion forming method according to technical solution 1 carries out vacuumize process
When, the pressure in die cavity is evacuated to 0.1~0.5MPa, preferably 0.1~0.2MPa.
8, a kind of high temperature resistant composite is made using any one of technical solution 1 to 7 forming method.
9, the high temperature resistant composite according to technical solution 8, the structure of the composite material are cell type.
10, the high temperature resistant composite according to technical solution 9, the composite material include built-in type cell type skeleton knot
Structure and the outer layer covering for being coated on the built-in type skeleton structure outer layer.
Beneficial effect
Above-mentioned technical proposal of the invention has the advantages that
(1) present invention can provide the thermal expansion pressure of stable and uniform using fluorubber as expanding material under the high temperature conditions
Power provides reliable process for the molding of fire resistant resin based composites.
(2) present invention passes through what is generated after calculating fluorubber expanded by heating using thermostable fluorine rubber as core model material
The determination of thermal expansion force and process gap, solves under the high temperature conditions that traditional silicon ageing of rubber causes the bulbs of pressure to reduce,
Solidifying pressure not enough causes product the defects of loose occur.Compared with traditional handicraft, it is multiple that fluorubber thermally expands molding high temperature resistant
Function admirable, the simple process of condensation material casing member form certain advantage to complex composite material.
(3) present invention is not necessarily to external pressure source, and heating equipment is heated using baking oven, and equipment investment is few, and manufacturing cost is low.
(4) present invention process can generate comprehensive, multi-angle enough pressure in pressure range, and it is whole to be suitable for Multicarity
The co-curing of body high temperature resistant composite product forms.
Detailed description of the invention
Fig. 1 is the flow diagram of forming method provided by the invention；
Fig. 2 is the structural schematic diagram of high temperature resistant composite cell type component.
Specific embodiment
To make the object, technical solutions and advantages of the present invention clearer, below in conjunction with the embodiment of the present invention, to this hair
Bright technical solution is clearly and completely described.Obviously, described embodiment is a part of the embodiments of the present invention, and
The embodiment being not all of.Based on the embodiments of the present invention, those of ordinary skill in the art are not making creative work
Under the premise of every other embodiment obtained, shall fall within the protection scope of the present invention.
The present invention provides a kind of high temperature resistant composite high-temperature heat expansion forming methods, as shown in Figure 1, high warm is swollen
Swollen forming method (abbreviation forming method) includes the following steps:
(1) prepare fluorubber core model: fluorubber and vulcanizing agent being uniformly mixed, deaeration is configured to glue；According to component knot
Structure design requirement processes the master mold of soft mode；Glue is poured into master mold to vulcanize, obtains fluorubber core model；
Vulcanizing agent additive amount is more, and sulphidity is higher in mixing process at a certain temperature for fluorubber, in high temperature and more sulphur
Cause sulfidation reaction that incipient scorch phenomenon, vulcanizing agent adding too much or mixing temperature excessively acutely can even occur under agent state
Height is spent, vulcanizable fluororubber degree increases, causes to be difficult to be shaped to suitable thickness, and fluorubber chemical inertness is stronger, while after
Phase is difficult and fiber carrier and structural film adhesive compoiste adhering；Vulcanizing agent additive amount is very little, and vulcanizable fluororubber degree is too low, in the later period
During co-curing, vulcanizable fluororubber is incomplete, influences hot expansibility.Based on above-mentioned consideration, in molding provided by the invention
In method, the mass ratio of the fluorubber and the vulcanizing agent is 100:(6~10), i.e. the additive amount (in mass) of vulcanizing agent
Be the 6~10% of fluorubber quality, for example, 6%, 6.1%, 6.2%, 6.3%, 6.4%, 6.5%, 6.6%, 6.7%,
6.8%, 6.9%, 7%, 7.1%, 7.2%, 7.3%, 7.4%, 7.5%, 7.6%, 7.7%, 7.8%, 7.9%, 8%,
8.1%, 8.2%, 8.3%, 8.4%, 8.5%, 8.6%, 8.7%, 8.8%, 8.9%, 9%, 9.1%, 9.2%, 9.3%,
9.4%, 9.5%, 9.6%, 9.7%, 9.8%, 9.9%, 10%.
Preferably, the fluorubber uses fluorine silicone rubber and/or fluoroether rubber.When fluorubber is fluorine silicone rubber and/or fluorine
When ether rubber, preferably at 120~150 DEG C (for example, can be 120 DEG C, 125 DEG C, 130 DEG C, 135 DEG C, 140 DEG C, 145 DEG C, 150
DEG C) carry out the vulcanization.For vulcanization time, to obtain the fine and close smooth superficial layer of fluorubber, and it is in suitable in resin
Core model is set to generate sufficiently large pressure when pressure point, according to formula P=k αR·(t-t0), k is tensile modulus of elasticity, and α is cubical expansion
Coefficient, it is preferred that the pressure limit generated after the expansion of resin pressure point, which is 18~20MPa,.Consider further that fluorubber thermal conductivity
It is low, therefore vulcanization time is determined as 60~80 minutes, uniform and stable temperature field could be generated, otherwise vulcanization is uneven, nothing
Method generates uniform thermal expansion stresses.
Preferably, the vulcanizing agent is using the peroxide that can carry out cross-linking reaction with fluorubber at 80 DEG C or less；It is preferred that
Ground, the vulcanizing agent are selected from cumyl peroxide, peroxidating bis- (2,4- dichloro-benzoyls), dibenzoyl peroxide, double uncles
Butyl peroxy cumene, triallyl isocyanate are any one or more of.
(2) prepreg is processed into prefabricated component, places the preform between fluorubber core model and former, determines technology room
Then gap molds, fastening；For process gap, the present invention is preferably 1.3~1.5mm.Fluorubber energy at 310 DEG C -330 DEG C
Enough briquetting pressures are enough provided, while excessive gummosis will not be caused, are combined between each layer preferable.With technology room
Downward trend after first rising is presented in the increase tensile strength modulus of gap.When process gap is less than 1.3mm, resin has just reached glutinous stream
When state does not have started solidification, fluorubber causes glue to be lost and generates poor glue with regard to premature offer pressure.Process gap is larger
When, the pressure that fluorubber generates component drastically reduces, and enough pressure cannot be provided in gelling temp, component is caused to generate
Layering.
In some embodiments, the prepreg includes resin matrix and fibre reinforcement；Preferably, the resin matrix
It is any one or more of selected from High temperature epoxy resins, cyanate resin, bimaleimide resin, polyimide resin；It is excellent
Selection of land, the fibre reinforcement is in carbon fibre fabric, glass fabric, quartz textile, carbon fiber, glass fibre
It is any one or more.
(3) vacuumize process is carried out to the die cavity of mold and prefabricated component therein, it is preferred for being evacuated to 0.1~0.5MPa
, then more preferably 0.1~0.2MPa carries out heating and thermal insulation to mold, is finally solidified, it is compound to obtain the high temperature resistant
Material.In this step, corresponding temperature and time can be maintained according to the cure parameter of resin, completes product solidification.
The present invention also provides a kind of high temperature resistant composites, are made using above-mentioned forming method.In some embodiments,
The structure of the composite material is cell type, and structure includes built-in type cell type skeleton structure and is coated on the built-in type skeleton knot
The outer layer covering of structure outer layer, as shown in Figure 2.Built-in type skeleton is primarily subjected to in-plane bending and shear-type load, and outer layer covering will divide
The built-in type skeleton of block is connected to become an overall structure.The cell type beam uses high-temperature heat expansion technological forming, and heat expansion material is resistance to
High temperature fluorubber mold, rigid material are former, and high temperature resistant composite is placed between core model and former, after mold is heated, by
It is limited in the volume expansion of core model by former and generates pressure in die cavity, realize adding in composite material solidification process
Pressure.
In order to clearly be illustrated, the preparation method of high temperature resistant composite cell type component can be according to such as lower section
It is prepared by method:
(1) prepare fluorubber core model: fluorubber and vulcanizing agent being uniformly mixed, deaeration is configured to glue；According to component knot
Structure design requirement processes the master mold of soft mode；Glue is poured into master mold to vulcanize, obtains fluorubber core model；Wherein, the fluorine
The mass ratio of rubber and the vulcanizing agent is 100:(7~10)；
(2) prepreg is processed into boxing prefabricated component, places the preform between fluorubber core model and former, determines technique
Then gap molds, fastening；
(3) vacuumize process is carried out to the die cavity of mold and prefabricated component therein, heating and thermal insulation then is carried out to mold,
Finally solidified, obtains the high temperature resistant composite.
Preferably: the fluorubber uses fluorine silicone rubber and/or fluoroether rubber.More preferably: being carried out at 120~150 DEG C
The vulcanization, time controlled at 60~80 minutes.
Preferably: the vulcanizing agent is using the peroxide that can carry out cross-linking reaction with fluorubber at 80 DEG C or less；It is preferred that
Ground, the vulcanizing agent are selected from cumyl peroxide, peroxidating bis- (2,4- dichloro-benzoyls), dibenzoyl peroxide, double uncles
Butyl peroxy cumene, triallyl isocyanate are any one or more of.
Preferably: the process gap is 1.3~1.5mm.
Preferably: the prepreg includes resin matrix and fibre reinforcement；
Preferably, the resin matrix is selected from High temperature epoxy resins, cyanate resin, bimaleimide resin, polyamides
Imide resin is any one or more of；
Preferably, the fibre reinforcement be selected from carbon fibre fabric, glass fabric, quartz textile, carbon fiber,
Glass fibre is any one or more of.
Preferably: when carrying out vacuumize process, the pressure in die cavity is evacuated to 0.1~0.5MPa, preferably 0.1~
0.2MPa。
Preferably, the cell type prefabricated component can carry out as follows processing and fabricating:
(a) prepreg is subjected to laying, is then cut according to case type structures, form built-in type cell type skeleton structure；
(b) multiple built-in type cell type skeleton structures are overlapped, then outer layer integral coating outer layer covering to get arrive box
Type prefabricated component.The fabric prepreg that outer layer covering can be formed using fabric and resin compounded, fabric can be with
Select carbon fibre fabric, glass fabric or quartz textile, resin that can select High temperature epoxy resins, cyanate ester tree
Rouge, bimaleimide resin, polyimide resin are any one or more of.
It is the embodiment that the present invention enumerates below.
Embodiment 1
An advanced High Temperature Resistant Polyimide Composites cell type component is made, composite material cell type component length is 300mm, wide
Spend 100mm, height 25mm, wall thickness 3mm.
Cell type component is pre- at 0.5mm thickness by { 45/0/-45/90 } sequence laying using polyimide carbon fiber prepreg
Leaching material is generated blanking template according to case type structures and is cut out using automatic fabric cutter, formed built-in type skeleton structure, bury interior
Formula skeleton structure superposition, recycle carbon fibre fabric prepreg integral coating, finally using fluorubber core model high-temperature heat expansion at
Type.Curing process is 240 DEG C of heat preservations 2h, 300 DEG C of heat preservation 1h, and then 370 DEG C of solidification 2h, demoulding form integrated cell type component.
Specific implementation process is as follows:
Uniform 3F board FE-2602 fluorubber and peroxidating bis- (2,4 dichloro benzene formyl) (i.e. vulcanizing agents) mixing will be kneaded
Uniformly, de-bubble processing is carried out using vacuum defoamation, preparation obtains glue；The mass ratio of the fluorubber and the vulcanizing agent is
100:6；The master mold of soft mode is processed according to element structure design requirement；Glue is poured into master mold to vulcanize, is 150 in temperature
Fluorubber core model is molded after vulcanizing 70 minutes in DEG C baking oven.
Using polyimide carbon fiber prepreg by { 45/0/-45/90 } sequence laying at 0.5mm prepreg thickness material, with certainly
Dynamic fabric cutter is cut into several sub-blocks according to case type structures shape, and together by 50 sub-block layings, forming theoretical level is
The hinge structure area preform of 25mm.Lateral wall forms cell type with carbon fibre fabric prepreg integral coating with a thickness of 3mm
Member preform.
Cell type member preform is fitted into mold, fluorubber core model, process gap 1.3mm, box are placed on the inside of component
Type component is integrally closed with metal die cavity.
Die cavity and prefabricated component therein are carried out being evacuated to 0.1MPa, mold temperature is risen into 240 DEG C of heat preservations by room temperature
2h, then 300 DEG C of heat preservation 1h are warming up to, then heat to 370 DEG C of solidification 2h.It is realized using the thermal expansion force of fluorubber to cell type part
The uniform pressurization of inner wall.
It is demoulded after cooling, obtains high temperature resistant composite cell type component.The discovery of this nondestructiving detecting means, box are swept using C
Type component inside quality is intact, does not occur loose equal part layer defects.
Embodiment 2
High temperature resistant cyanate resin composite material flat plate formula component is prepared, composite material flat plate formula component length is 300mm,
Width is 100mm, with a thickness of 20mm.
Qualified size is cut into using cyanate ester resin carbon fiber prepreg, laying stacks, and forms flat prepreg, adopts
It is formed with fluorubber core model high-temperature heat expansion.Curing process is 220 DEG C of heat preservations 2h, 280 DEG C of heat preservation 1h, then 350 DEG C of solidification 2h,
Demoulding forms integrated component.Specific implementation process is as follows:
Uniform 3F board FE-2602 fluorubber and peroxidating bis- (2,4 dichloro benzene formyl) (i.e. vulcanizing agents) mixing will be kneaded
Uniformly, de-bubble processing is carried out using vacuum defoamation, preparation obtains glue；The mass ratio of the fluorubber and the vulcanizing agent is
100:7；The master mold of soft mode is processed according to element structure design requirement；Glue is poured into master mold to vulcanize, is 150 in temperature
Cell type fluorubber core model is molded after vulcanizing 70 minutes in DEG C baking oven.
Cyanate carbon fiber prepreg is cut out into qualified size size, together by multilayer prepreg laying, formation can obtain
The preform that theoretic throat is 20mm is obtained, as prefabricated component.
Prefabricated component is coated in fluorubber mandrel surface, process gap 1.3mm, it is whole to be closed with metal die cavity.
Die cavity and prefabricated component therein are carried out being evacuated to 0.1MPa, mold temperature is risen into 220 DEG C of heat preservations by room temperature
2h, then 280 DEG C of heat preservation 1h are warming up to, then heat to 350 DEG C of solidification 2h.It is realized using the thermal expansion force of fluorubber to prefabricated component
The uniform pressurization of inner wall.
It is demoulded after cooling, obtains high temperature resistant composite flat component.The discovery of this nondestructiving detecting means is swept using C,
Cell type component inside quality is intact, does not occur loose equal part layer defects.
Finally, it should be noted that the above embodiments are merely illustrative of the technical solutions of the present invention, rather than its limitations；Although
Present invention has been described in detail with reference to the aforementioned embodiments, those skilled in the art should understand that: it still may be used
To modify the technical solutions described in the foregoing embodiments or equivalent replacement of some of the technical features；
And these are modified or replaceed, technical solution of various embodiments of the present invention that it does not separate the essence of the corresponding technical solution spirit and
Range.
Claims (10)
1. a kind of high temperature resistant composite high-temperature heat expansion forming method, characterized by the following steps:
(1) prepare fluorubber core model: fluorubber and vulcanizing agent being uniformly mixed, deaeration is configured to glue；It is set according to element structure
Meter requires to process the master mold of soft mode；Glue is poured into master mold to vulcanize, obtains fluorubber core model；Wherein, the fluorubber
Mass ratio with the vulcanizing agent is 100:(7~10)；
(2) prepreg is processed into prefabricated component, placed the preform between fluorubber core model and former, determine process gap, so
After mold, fasten；
(3) vacuumize process is carried out to the die cavity of mold and prefabricated component therein, heating and thermal insulation then is carried out to mold, finally
Solidified, obtains the high temperature resistant composite.
2. high temperature resistant composite high-temperature heat expansion forming method according to claim 1, it is characterised in that: the fluorine rubber
Glue uses fluorine silicone rubber and/or fluoroether rubber.
3. high temperature resistant composite high-temperature heat expansion forming method according to claim 2, it is characterised in that: 120~
150 DEG C carry out the vulcanization, and the time controlled at 60~80 minutes.
4. high temperature resistant composite high-temperature heat expansion forming method according to any one of claims 1 to 3, feature exist
In: the vulcanizing agent is using the peroxide that can carry out cross-linking reaction with fluorubber at 80 DEG C or less；Preferably, the vulcanizing agent
Selected from cumyl peroxide, peroxidating bis- (2,4 dichloro benzene formyls), dibenzoyl peroxide, double tert-butyl peroxy isopropyls
Benzene, triallyl isocyanate are any one or more of.
5. high temperature resistant composite high-temperature heat expansion forming method according to claim 1, it is characterised in that: the technique
Gap is 1.3~1.5mm.
6. high temperature resistant composite high-temperature heat expansion forming method according to claim 1, it is characterised in that: the preimpregnation
Material includes resin matrix and fibre reinforcement；Preferably, the resin matrix is selected from High temperature epoxy resins, cyanate resin, double
Maleimide resin, polyimide resin are any one or more of；Preferably, the fibre reinforcement is knitted selected from carbon fiber
Object, glass fabric, quartz textile, carbon fiber, glass fibre are any one or more of.
7. high temperature resistant composite high-temperature heat expansion forming method according to claim 1, it is characterised in that: take out true
When vacancy is managed, the pressure in die cavity is evacuated to 0.1~0.5MPa, preferably 0.1~0.2MPa.
8. a kind of high temperature resistant composite, it is characterised in that: be made using any one of claim 1 to 7 forming method.
9. high temperature resistant composite according to claim 8, it is characterised in that: the structure of the composite material is cell type.
10. high temperature resistant composite according to claim 9, it is characterised in that: the composite material includes built-in type box
Type skeleton structure and the outer layer covering for being coated on the built-in type skeleton structure outer layer.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111688238A (en) * | 2020-05-27 | 2020-09-22 | 长春三友智造科技发展有限公司 | Method for forming thermosetting polymer fiber composite material part |
| CN113561522A (en) * | 2021-07-19 | 2021-10-29 | 南京航空航天大学 | Three-dimensional woven fiber reinforced honeycomb preparation device and method based on thermal expansion flexible core mold |
| CN113696499A (en) * | 2021-08-26 | 2021-11-26 | 航天特种材料及工艺技术研究所 | Preparation method of assembled anti-deformation lightweight carbon fiber composite material frame |
| CN117656538A (en) * | 2024-02-02 | 2024-03-08 | 哈尔滨远驰航空装备有限公司 | Forming die and forming method for special-shaped hollow pipe fitting |
| CN117727405A (en) * | 2024-02-08 | 2024-03-19 | 北京理工大学 | Method and device for analyzing interaction of soft mold-composite material grid structure |
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| JPS59188405A (en) * | 1983-04-11 | 1984-10-25 | Nitto Electric Ind Co Ltd | Manufacture of heat-shrinkable hollow body |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111688238A (en) * | 2020-05-27 | 2020-09-22 | 长春三友智造科技发展有限公司 | Method for forming thermosetting polymer fiber composite material part |
| CN113561522A (en) * | 2021-07-19 | 2021-10-29 | 南京航空航天大学 | Three-dimensional woven fiber reinforced honeycomb preparation device and method based on thermal expansion flexible core mold |
| CN113696499A (en) * | 2021-08-26 | 2021-11-26 | 航天特种材料及工艺技术研究所 | Preparation method of assembled anti-deformation lightweight carbon fiber composite material frame |
| CN113696499B (en) * | 2021-08-26 | 2023-09-15 | 航天特种材料及工艺技术研究所 | Preparation method of assembled deformation-preventing light-weight carbon fiber composite material frame |
| CN117656538A (en) * | 2024-02-02 | 2024-03-08 | 哈尔滨远驰航空装备有限公司 | Forming die and forming method for special-shaped hollow pipe fitting |
| CN117656538B (en) * | 2024-02-02 | 2024-04-26 | 哈尔滨远驰航空装备有限公司 | Forming die and forming method for special-shaped hollow pipe fitting |
| CN117727405A (en) * | 2024-02-08 | 2024-03-19 | 北京理工大学 | Method and device for analyzing interaction of soft mold-composite material grid structure |
| CN117727405B (en) * | 2024-02-08 | 2024-04-30 | 北京理工大学 | Method and device for analyzing interaction of soft mold-composite material grid structure |
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